HRID1748591

反应详情

EQUATION

反应方程式

HRID 1748591 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To N-[6-(1-tert-butyloxycarbonylpiperidin-4-yl)-5-methylpyridin-3-yl]-5-methyl-1-[5-(trifluoromethyl)pyridin-2-yl]-1H-pyrazole-4-carboxamide (7.0 g) were added dichloromethane (128 ml) and trifluoroacetic acid (26 ml), stirred at room temperature for 2 hours, and then to the reaction solution was added 4 N aqueous solution of sodium hydroxide under ice-cooling. The precipitated solid was washed with n-hexane and water, the obtained solid was dissolved in chloroform, water was added thereto, extracted with chloroform and ethyl acetate, dried over anhydrous sodium sulfate, and then the solvent was evaporated in vacuo. The precipitated solid was washed with ethyl acetate to give the titled compound (5.39 g) as a white solid.

WORKUP

后处理

  1. temperaturecooling
  2. washThe precipitated solid was washed with n-hexane and water
  3. dissolutionthe obtained solid was dissolved in chloroform
  4. additionwater was added
  5. extractionextracted with chloroform and ethyl acetate
  6. dry with materialdried over anhydrous sodium sulfate
  7. customthe solvent was evaporated in vacuo
  8. washThe precipitated solid was washed with ethyl acetate